N-甲基吡咯烷酮硫酸氢盐催化合成7-羟基-4-甲基香豆素  

Synthesis of 7-hydroxy-4-methylcoumarin catalyzed by 1-methyl-2-pyrrolidinone hydrosulfate

作　　者：滕俊江[1] 乔艳辉[1] 林培喜[1] 

机构地区：[1]广东石油化工学院化学与生命科学学院,广东茂名525000

出　　处：《化工进展》2012年第6期1321-1324,共4页Chemical Industry and Engineering Progress

基　　金：茂名市重点科技计划项目(10A18)

摘　　要：以离子液体N-甲基吡咯烷酮硫酸氢盐为催化剂,通过Pechmann缩合反应于无溶剂条件下合成了7-羟基-4-甲基香豆素,实验表明N-甲基吡咯烷酮硫酸氢盐可重复使用并具有较好的催化活性。在原料摩尔比n(间苯二酚)∶n(乙酰乙酸乙酯)为1∶1.3、催化剂[Hnmp]HSO4占反应物料总质量的1.2%、回流反应时间3 h的条件下,产品收率达87.24%,经液相色谱分析纯度大于98.5%。7-Hydroxy-4-methylcoumarin was synthesized by Pechmann reaction using ionic liquid 1-methyl-2-pyrrolidinone hydrosulfate as catalyst without solvent.The results showed that 1-methyl-2-pyrrolidinone hydrosulfate could be reused and exhibited excellent catalytic activity.Under the condition as：n（resorcinol）∶n（ethyl acetoacetate）=1∶1.3,1.2%（percent of total mass of reactants） HSO4,refluxing for 3 h,the yield of 7-hydroxy-4-methylcoumarin is up to 87.24%.Purity of product analyzed by HPLC is above 98.5%.

关 键 词：N-甲基吡咯烷酮 硫酸氢盐 7-羟基-4-甲基香豆素 合成 

分 类 号：TQ203.2[化学工程—有机化工]